高效液相色谱法检测菜豆中阿维菌素残留量

张儒令 安凤颖 胡德禹 张钰萍 张侃侃 卢平

摘要    本文建立了反相高效液相色譜法测定菜豆中阿维菌素残留量的方法，即以乙酸乙酯为提取剂，液液萃取净化，经N-甲基咪唑和三氟醋酸酐衍生化，采用高效液相色谱法-荧光检测器（激发波长365 nm，发射波长470 nm）进行测定。同时，为了确定1%阿维菌素水乳剂在菜豆中的施用安全性，通过2年两地田间试验和样品室内检测试验，研究了其在菜豆上的消解动态及最终残留量。结果表明，在0.050～5.000 μg/mL浓度范围内，阿维菌素的浓度与峰面积线性关系良好，线性相关系数γ=0.999 3。添加浓度在0.004 4～0.440 0 mg/kg时，方法的平均回收率为94.35%～99.42%，相对标准偏差为4.81%～5.84%;以1%阿维菌素水乳剂0.45 g/m2喷药，阿维菌素在菜豆上的消解半衰期为1.4～1.7 d;施药7 d后采集的菜豆样品中阿维菌素含量均低于MRL值0.05 mg/kg。本方法简便、快速、准确，适用于阿维菌素在菜豆上的残留量测定。

关键词    阿维菌素;菜豆;残留;消解动态;高效液相色谱法

中图分类号    S481+.8        文献标识码    A

文章编号   1007-5739（2020）06-0106-03                                                                                     开放科学（资源服务）标识码（OSID）

Determination  of  Abamectin  Residue  in  Kidney  Bean  by  HPLC

ZHANG Ru-ling 1    AN Feng-ying 1    HU De-yu 2 *    ZHANG Yu-ping 2    ZHANG Kan-kan 2    LU Ping 2

（1 Tongren Vocational and Technical College，Tongren Guizhou 554300; 2 Research and Development Cnter for Fine Chemicals，Guizhou University）

Abstract    A reversed-phase HPLC method for the determination of avermectin residues in kidney bean was established.The avermectin residues in kidney bean were extracted and purified by liquid-liquid extraction with ethyl acetate as the extractant.After derivatization with N-methylimidazole and trifluoroacetic anhydride，the avermectin residues in kidney bean were determined by HPLC with fluorescence detector（excitation wavelength was 365 nm and emission wavelength was 470 nm）.At the same time，the digestion dynamics and the final residue of abamectin water emulsion in kidney bean were studied through two years of two fields test and sample laboratory test，in order to determine the application safety of 1% abamectin water emulsion in kidney bean.The results showed that in the range of 0.050-5.000 μg/mL，the linear relationship between avermectin concentration and peak area was good，and the linear correlation coefficient was 0.999 3.When the concentration was 0.004 4-0.440 0 mg/kg，the average recovery of the method was 94.35%-99.42%，and the relative standard deviation was 4.81%-5.84%.When the 1% abamectin water emulsion was 0.45 g/m2，the half-life of abamectin digestion on kidney bean was 1.4-1.7 d.The content of abamectin in kidney bean samples collected after 7 days was lower than that of MRL 0.05 mg/kg.This method is simple，rapid and accurate.It is suitable for the determination of avermectin residue in kidney bean.

Key words    abamectin;kidney bean;residue;digestion dynamic;HPLC

阿维菌素是一类具有杀虫、杀螨、杀线虫活性的十六元环内酯双糖类化合物，是经过微生物发酵、提取的新型抗生素类杀虫杀螨剂[1-7]，对多种作物的害虫和螨类具有触杀和胃毒作用，同时具有微弱的熏蒸作用，无内吸作用[8-10]，具有广谱、高效、低残留等特点，不易对土壤各种微生物和各种酶产生较大危害[11]，是当前农业害虫综合防治中理想的生物农药[12]。

关于阿维菌素的检测方法国内外有大量报道，张少华等[13]建立了以乙腈为提取溶剂，测定葱中阿维菌素残留。……